CN114956898A - Nitrogen-fixing fertilizer-maintaining synergist, self-assembly nitrogen-containing fertilizer containing nitrogen-fixing fertilizer-maintaining synergist and preparation method of self-assembly nitrogen-containing fertilizer - Google Patents

Nitrogen-fixing fertilizer-maintaining synergist, self-assembly nitrogen-containing fertilizer containing nitrogen-fixing fertilizer-maintaining synergist and preparation method of self-assembly nitrogen-containing fertilizer Download PDF

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CN114956898A
CN114956898A CN202210770792.5A CN202210770792A CN114956898A CN 114956898 A CN114956898 A CN 114956898A CN 202210770792 A CN202210770792 A CN 202210770792A CN 114956898 A CN114956898 A CN 114956898A
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nitrogen
fertilizer
synergist
fixing
polysuccinimide
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CN114956898B (en
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焦永康
范占权
赵龙梅
张阔
李华帅
刘双虎
崔晓明
李贺华
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Hebei Xieli Chemical Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C9/00—Fertilisers containing urea or urea compounds
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1092—Polysuccinimides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
    • Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures

Abstract

The invention discloses a nitrogen-fixing fertilizer-maintaining synergist which is an organic nitrogen source synergist and is mainly formed by reacting polysuccinimide and amide nitrogen, wherein the polymerization degree of the polysuccinimide is 15-80, and the mass of the polysuccinimide accounts for 20-80% of the total mass of the organic nitrogen source synergist. Meanwhile, the invention also discloses a self-assembly nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist, wherein each hundred parts of the nitrogen-containing fertilizer comprises 1-70 parts of the nitrogen-fixing and fertilizer-maintaining synergist. The obtained self-assembly nitrogen-containing fertilizer controls the reasonable release of nitrogen elements in the nitrogen-containing fertilizer by using the effective components of the synergist, reduces the loss of volatilization, leaching loss and the like of a conventional nitrogen source, obviously improves the comprehensive utilization rate of the fertilizer in the application process, and promotes the organic implementation of intensive agricultural production.

Description

Nitrogen-fixing fertilizer-maintaining synergist, self-assembly nitrogen-containing fertilizer containing nitrogen-fixing fertilizer-maintaining synergist and preparation method of self-assembly nitrogen-containing fertilizer
Technical Field
The invention relates to the technical field of fertilizer synergists and fertilizers, in particular to a nitrogen-fixing and fertilizer-maintaining synergist and a preparation method thereof, and a self-assembly nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist and a preparation method thereof.
Background
According to 2017 statistics of the food and agriculture organization of the united nations, the global food yield is about 26.27 hundred million tons, the Chinese food yield is 6.18 hundred million tons, and the total global food yield accounts for 23.5 percent in the same period. In order to maintain such high grain yield, a large amount of agricultural chemicals are consumed in the agricultural production process of China at present, wherein nitrogen fertilizers occupy an absolute amount. In 2017, the total application of the nitrogen fertilizer in China reaches 2220.6 ten thousand tons, which accounts for 35% of the total amount in the world, and although a plurality of novel fertilizers with certain nitrogen saving effect are included, such as polypeptide urea and sustained and controlled release urea with the weight of more than 300 ten thousand tons, the comprehensive utilization rate of the nitrogen fertilizer in China is still less than 35% in the current year, so that great waste is caused. Through analysis, experts consistently consider that improper fertilization method is the main cause of fertilizer waste, and the loss way mainly comprises the following steps: ammonia volatilization of ammonium nitrogen fertilizer (including volatilization of ammonia after urea conversion), direct leaching loss of nitrate nitrogen fertilizer and urea, and gaseous nitrogen loss caused by denitrification in paddy field. If the problems can be effectively solved, the method has great significance for the development of intensive agriculture.
Disclosure of Invention
In order to solve the defects of the prior art, the nitrogen-fixing and fertilizer-retaining synergist is used for adjusting the existence form and the release mode of nitrogen elements in the nitrogen fertilizer, so that the slow release rate and the comprehensive utilization rate of the nitrogen fertilizer are effectively improved, and the high-efficiency implementation of intensive agricultural production is promoted.
In order to achieve the purpose, the nitrogen-fixing fertilizer-retaining synergist provided by the invention is an organic nitrogen source synergist and is mainly formed by reacting polysuccinimide and amide nitrogen, wherein the polymerization degree of the polysuccinimide is 15-80, and the mass of the polysuccinimide accounts for 20-80% of the total mass of the organic nitrogen source synergist. .
According to the invention, the organic nitrogen source synergist containing a biuret-like structure, which is obtained by reacting polysuccinimide with amide nitrogen, is used for promoting the organization of free nitrogen in a nitrogen-containing fertilizer system, and through the combined action of microorganisms in the environment and the pH value of soil, the organic nitrogen source synergist is slowly released in a chain scission manner, so that the supply of nitrogen elements required by crops in the whole growth process is met, the losses such as volatilization, leaching loss and the like existing in the conventional nitrogen source are reduced, the utilization rate of nitrogen fertilizer is effectively improved, the application amount is reduced, the purposes of energy conservation, emission reduction and carbon emission reduction are really achieved, and the organic implementation of intensive agricultural production is promoted.
As a limitation to the above technical means, the polysuccinimide is obtained by polymerizing at a temperature of 180 to 300 ℃ by a thermal aspartic acid polymerization method, a thermal maleic acid ammonium salt polymerization method or a thermal fumaric acid ammonium salt polymerization method.
For the selection of polysuccinimide, it is generally required that the residual amount of the corresponding starting material in polysuccinimide is 2% or less.
Polysuccinimide obtained by an aspartic acid (comprising L-aspartic acid, D-aspartic acid and D, L-aspartic acid) thermal polymerization method or a maleic acid ammonium salt thermal polymerization method or a fumaric acid ammonium salt thermal polymerization method is added into a melting system of amide nitrogen, insoluble impurities cannot occur or few insoluble impurities occur, so that the problem that the content of water insoluble substances in a subsequent organic nitrogen fertilizer is too high is avoided; meanwhile, the polysuccinimide obtained from the raw materials has moderate polymerization degree, so that the processed nitrogen fertilizer not only ensures the lasting effect, but also keeps a part of quick-acting property, thereby prolonging the time of the nitrogen supply of the fertilizer to crops.
In terms of polymerization degree, the polymerization degree of polysuccinimide obtained by thermal polymerization of aspartic acid (including L-aspartic acid, D-aspartic acid and D, L-aspartic acid) is in the range of 15 to 80, while the polymerization degree of polysuccinimide obtained by thermal polymerization of ammonium maleate or ammonium fumarate is mostly in the range of 15 to 50.
If the polymerization degree needs to be improved continuously, a certain catalyst is added in the process of synthesizing the polysuccinimide, and the catalyst generally takes phosphoric acid and derivatives thereof as main materials, so that the polymerization degree of the obtained polysuccinimide is generally greater than 85, but a part of water insoluble substances are formed in the process of producing organic nitrogen fertilizers, and meanwhile, the early effect of the organic nitrogen fertilizers is poor, so that the early stage of crops is lack of fertilizer supply, and physiological diseases are caused.
As a limitation to the above technical solution, the amide nitrogen is at least one selected from urea, urea-formaldehyde, crotonobiurea and amide. Wherein the urea comprises common urea, large granular urea containing formaldehyde, edible pigment, and novel urea/value-added urea containing conventional synergistic substances (humic acid, alginic acid, amino acids and their derivatives); the amide comprises one or more of formamide, acetamide and propionamide.
The amide nitrogen particularly takes urea, urea-formaldehyde, butylene diamine and amide as raw materials, and is more beneficial to carrying out high-efficiency and stable reaction with thermal polymerization polysuccinimide, and the organic slow-release nitrogen fertilizer synergist containing a biuret-like structure is stably formed; after the nitrogen-containing fertilizer is added, the obtained fertilizer can efficiently control the release rate of nitrogen, so that the utilization rate of the nitrogen is obviously improved.
As a limitation to the technical scheme, the organic nitrogen source synergist is mainly prepared by adding fluid polysuccinimide into molten amide nitrogen for reaction.
Meanwhile, the invention also provides a preparation method of the nitrogen-fixing fertilizer-retaining synergist, which is to prepare the raw material polysuccinimide into a non-layered fluid material, uniformly add the non-layered fluid material into the amide nitrogen in a molten state, keep the material completely reacted without obvious polysuccinimide and then mold the mixture to obtain the synergist.
The nitrogen-fixing fertilizer-retaining synergist is prepared by reacting fluid polysuccinimide with molten amide nitrogen, and an organic nitrogen synergist is obtained after the materials are completely reacted without obvious polysuccinimide, so that the nitrogen-fixing fertilizer-retaining synergist is more beneficial to the generation of a slow-release structure and the controlled release of nitrogen elements, and the weight-reducing and efficiency-increasing effects of the organic nitrogen source synergist are fully exerted.
As the limitation of the technical scheme, the fluid polysuccinimide is obtained by using water as a suspension medium and processing by using a colloid mill or a homogenizer; the mass ratio of the polysuccinimide to the water in the process of preparing the fluid polysuccinimide is 1 (0.25-2.50).
The polysuccinimide is uniformly dispersed in water to obtain a homogenized fluid raw material, which is favorable for reacting with molten amide nitrogen to prepare the organic nitrogen source synergist with a required slow-release structure.
The invention further provides a self-assembly nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist, namely, 1-70 parts of the nitrogen-fixing and fertilizer-maintaining synergist is contained in each hundred parts of the nitrogen-containing fertilizer.
As a limitation on the technical scheme, the nitrogen-containing fertilizer also comprises auxiliary materials, wherein the auxiliary materials comprise at least one of nitrification inhibitor, urease inhibitor and synergistic accelerator.
As a limitation on the technical scheme, the nitrification inhibitor is at least one of 2-chloro-6- (trichloromethyl) pyridine (CP) and 3, 4-dimethylpyrazole phosphate (DMPP), and each hundred parts of the nitrogen-containing fertilizer comprises 0.1-5.0 parts of the nitrification inhibitor;
the urease inhibitor is a phosphorus amine urease inhibitor, and each hundred parts of nitrogen-containing fertilizer comprises 0.5-5.0 parts of urease inhibitor;
the synergistic accelerator is at least one of allantoin, polyamine substances, oligosaccharins and jasmonic acid substances, and each hundred parts of nitrogen-containing fertilizer comprises 0.05-1.0 part of synergistic accelerator.
The nitrogen-fixing and fertilizer-maintaining synergist is matched with a common nitrogen-containing fertilizer and then acts with other auxiliary materials together, so that the self-assembly nitrogen-containing fertilizer with excellent effect is obtained. The auxiliary materials such as nitrification inhibitor, urease inhibitor, synergistic accelerator and the like are added, the adverse effects of soil environment on the slow release process of the organic nitrogen source in the nitrogen fertilizer and the effect of nitrogen elements after release are reduced, the comprehensive utilization rate of the nitrogen fertilizer is further improved, the application amount of the fertilizer is reduced, the cost is saved, the secondary pollution is reduced, and the improvement of the intensive agricultural production efficiency is promoted.
As a limitation on the technical scheme, the nitrogen-fixing and fertilizer-maintaining synergist and the auxiliary materials are uniformly stirred and added into the production process of the common nitrogen-containing fertilizer in proportion to obtain the self-assembly nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist.
The nitrogen-fixing and fertilizer-maintaining synergist and other auxiliary materials are uniformly stirred and then added into the fertilizer production process according to a proportion, after the nitrogen-containing fertilizer with higher utilization rate and high slow release performance is obtained through spraying granulation and molding, the materials automatically participate in the formation of the nitrogen-containing fertilizer by utilizing the wrapping, adhesion, reaction heat and the like of the nitrogen-containing fertilizer on the auxiliary materials, and finally the self-assembly nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist is obtained through molding.
The self-assembly nitrogen-containing fertilizer containing nitrogen-fixing and fertilizer-maintaining synergist utilizes the organic nitrogen source in a specific form as the synergist, controls the release rate of nitrogen element by the organic nitrogen source synergist and further cooperating with the combined action of auxiliary materials, reduces the loss of volatilization, leaching and the like of the conventional nitrogen source, truly exerts the weight-reducing and synergistic effects of the nitrogen-containing fertilizer, obviously improves the comprehensive utilization rate and reduces the application amount of the fertilizer in the application process, achieves the purposes of saving energy, reducing consumption and secondary pollution, and promotes the organic implementation of intensive agricultural production.
Drawings
FIG. 1 photograph of corn samples according to example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The following examples and comparative examples relate to drugs which are typical products purchased on the market.
Examples
The embodiment relates to a self-assembly nitrogen-containing fertilizer containing a nitrogen-fixing and fertilizer-maintaining synergist and preparation thereof.
Example 1
A self-assembly nitrogen-containing fertilizer containing nitrogen-fixing and fertilizer-maintaining synergist, namely a nitrogen-containing fertilizer-special urea I, is prepared according to the following method:
stirring is started in a 2L flask, 450g of water and 550g of polysuccinimide are added at one time, the polysuccinimide is obtained by an L-aspartic acid thermal polymerization method (the thermal polymerization temperature is 240 +/-5 ℃, the thermal polymerization time is 4 hours), the polymerization degree is 50, the content of free aspartic acid is less than 0.5 percent, after the polysuccinimide and the water are uniformly stirred, the polysuccinimide and the water are transferred to a colloid mill by a pouring method, the mixed material is ground by a wet grinding method under the condition of 8000-10000 r/min for 60 minutes, the material is a non-layered suspending agent, the particle size of the material is less than or equal to 5 mu m measured by a laser particle sizer, and the solid content of the material is 55 percent.
Uniformly pumping the suspending agent into molten urea (urea is an amide nitrogen source of the synergist and accounts for 40% of the mass of the synergist) according to the mass of the polysuccinimide accounting for 60% of the mass of the synergist, and keeping the reaction temperature of the materials at 100-135 ℃ until no polysuccinimide particles exist in the system to obtain the organic nitrogen source synergist for producing the special urea I; the synergist is added into molten urea slurry (namely the production raw material of the conventional nitrogen fertilizer urea) for spraying granulation after 20 kg/ton of the synergist, 1.0 kg/ton of 2-chloro-6- (trichloromethyl) pyridine (CP) and 0.5 kg/ton of allantoin are uniformly stirred, so as to form the special urea I. 45.50 percent of total nitrogen in the special urea I conforms to the relevant regulation of the national standard GB/T2440-2017 urea; it also contains 1.2% protein-bound nitrogen (the detection method is described in GB5009.5-2010 for protein determination, the same applies below), 0.1% CP, and 0.05% allantoin.
The special urea I prepared in the example 1 is subjected to a field test, the special urea I is applied to topdressing of summer corns in a constant fertilization mode of 15 kg/mu and a decrement fertilization mode of 12 kg/mu, meanwhile, the topdressing amount of the common urea is set to be 15 kg/mu as a control, each treatment is repeated for 3 times, and the area of each cell is 300m 2 Each cell performs a random block. In the test, the Yuanshi county (the east longitude is 114 degrees, 52 degrees and the northern latitude is 37 degrees, 75') of the Hebei Shijiazhuang is selected; the experimental time is from the large flare-out period of summer corn to corn harvesting, the yield is independently determined by adopting each cell, and the nitrogen utilization rate in the determined project is determined by the content and use of total nitrogen in corn plantsThe mass calculation of pure nitrogen in the nitrogenous fertilizer is carried out, wherein the nitrogen is measured according to the relevant regulations in the measurement of the total nitrogen, phosphorus and potassium contents of NY/T1977-2010 water-soluble fertilizer, the enzyme activity relevant measurement is carried out according to the relevant regulations of plant physiological and biochemical experimental principles and technologies (second edition), other indexes are designed and analyzed according to the relevant requirements of common general agricultural theories, the effect verification of the special urea I is carried out by a comprehensive statistical analysis method, the SPSS20.0 data analysis system is used for carrying out single-factor analysis of variance, and the Dunckan method is used for carrying out the difference significance test; the results of the combined data are shown in Table 1 below.
Figure BDA0003724133150000061
Figure BDA0003724133150000071
In the experimental years of the attached drawings, the pollination of the corn is influenced by large rainwater in the pollination period of the corn, so that the empty ear rate is higher, but the empty ear phenomenon does not occur in the treatment by using the synergist; there are two reasons analyzed: after the special urea is used, the nitrogen is supplied in a continuous supply state, so that the metabolism of elements related to the nitrogen metabolism, such as iron, zinc, copper and the like, keeps higher activity, and the shortage of pollination is reduced; secondly, nitrogen synergists, synergists and the like in the special fertilizer have the characteristic of strong stimulation of root system growth, promote the great development of the root system, enable crops to better utilize the nutrition in the soil and further reduce the rate of empty spikes.
Example 2
A self-assembly nitrogen-containing fertilizer containing nitrogen-fixing fertilizer-preserving synergist, namely a nitrogen-containing fertilizer-special urea II, is prepared according to the following method:
stirring is started in a 2L flask, 500g of water and 500g of polysuccinimide are added at one time, the polysuccinimide is obtained by an L-aspartic acid thermal polymerization method (the thermal polymerization temperature is 250 +/-5 ℃, the thermal polymerization time is 6 hours), the polymerization degree is 75, the content of free aspartic acid is less than 0.5 percent, the mixture is transferred to a colloid mill by a pouring method after being uniformly stirred, the mixture is ground for 75 minutes by a wet grinding method under the condition of 8000-10000 r/min, the material is a non-layering suspending agent, the particle size of the material is less than or equal to 5 mu m measured by a laser particle sizer, and the solid content of the material is 50 percent.
Uniformly pumping the suspending agent into molten urea formaldehyde (urea formaldehyde is an amide nitrogen source of the synergist and accounts for 45% of the mass of the synergist) according to the mass of the polysuccinimide which accounts for 55% of the mass of the synergist, and keeping the reaction temperature of the materials at 100-135 ℃ until no obvious polysuccinimide particles exist in the system to obtain the organic nitrogen source synergist for producing the special urea II; the synergist is added into molten urine for spraying granulation after being evenly stirred according to 50 kg/ton of synergist, 3.0 kg/ton of 3, 4-dimethylpyrazole phosphate (DMPP) and 0.5 kg/ton of allantoin to form the special urea II. The total nitrogen content of the special urea II is 45.20 percent, and the special urea II meets the relevant regulation of the national standard GB/T2440-2017 urea; meanwhile, the composition contains 2.75% of protein-bound nitrogen, 0.3% of DMPP and 0.05% of allantoin.
The special urea II prepared in the example 2 is subjected to a field test, the special urea II is applied to topdressing of summer corns in a constant fertilization rate of 15 kg/mu and a decrement fertilization rate of 12 kg/mu, meanwhile, a common urea topdressing amount of 15 kg/mu is set as a reference, and the test conditions, the operation, the data statistics and the analysis method are the same as those of the example 1; the results after combining the data are shown in Table 2 below.
Figure BDA0003724133150000081
Example 3
A self-assembly nitrogen-containing fertilizer containing nitrogen-fixing fertilizer-preserving synergist, namely a nitrogen-containing fertilizer-special ammonium sulfate III, is prepared according to the following method:
in a 2000L reaction kettle, stirring is started, 1000kg of water and 1200kg of polysuccinimide are added at one time, wherein 800kg of polysuccinimide and 400kg of polysuccinimide are obtained by a D, L-aspartic acid thermal polymerization method (the thermal polymerization temperature is 220 +/-10 ℃ and the thermal polymerization time is 4-5 h), 400kg of polysuccinimide is obtained by a maleic acid (mono) ammonium thermal polymerization method, the average polymerization degree is 40 (polysuccinimide obtained by the D, L-aspartic acid thermal polymerization method and the maleic acid mono-ammonium thermal polymerization method with approximate polymerization degrees are mixed), the content of free aspartic acid is less than 1.0 percent, the mixture is transferred into a colloid mill by a pouring method after being stirred uniformly, the mixture is ground circularly by a wet grinding method for 2 times and total 80min under the condition of 8000-10000 r/min, the material is a non-layering suspending agent, the particle size of the material is less than or equal to 5 mu m measured by a laser particle sizer, and the solid content of the material is 54.50 percent.
Uniformly pumping the suspending agent into molten urea (urea is an amide nitrogen source of the synergist and accounts for 40% of the mass of the synergist) according to the mass of the polysuccinimide accounting for 60% of the mass of the synergist, and keeping the reaction temperature of the materials at 100-135 ℃ until no polysuccinimide particles exist in the system to obtain the organic nitrogen source synergist for producing the special ammonium sulfate III; the synergist is added into molten ammonium sulfate slurry (namely the production raw material of the conventional nitrogen fertilizer ammonium sulfate) for spray granulation after being uniformly stirred according to 15 kg/ton of the synergist, 1.0 kg/ton of 2-chloro-6- (trichloromethyl) pyridine (CP), 2.0 kg/ton of 3, 4-dimethylpyrazole phosphate (DMPP) and 0.75 kg/ton of allantoin to form the special ammonium sulfate III. The total nitrogen in the special ammonium sulfate III is 20.5 percent, and the special ammonium sulfate III conforms to the related regulation of the national standard GB535-1995 ammonium sulfate; simultaneously contains 0.89% of protein-bound nitrogen, 0.1% of CP, 0.2% of DMPP and 0.075% of allantoin.
The special ammonium sulfate III prepared in the embodiment 3 is subjected to a field test, the special ammonium sulfate III is applied to topdressing of summer corns in a constant fertilization amount of 30 kg/mu and a decrement fertilization amount of 24 kg/mu, and meanwhile, a common urea topdressing amount of 30 kg/mu is set as a reference, and the test conditions, the operation, the data statistics and the analysis method are the same as those of the embodiment 1; the results after combining the data are shown in Table 3 below.
Figure BDA0003724133150000091
Figure BDA0003724133150000101
The results of the above examples show that the self-assembly nitrogen-containing fertilizer synergist-containing self-assembly nitrogen-containing fertilizer of the present invention has the advantages of significantly improved nitrogen utilization rate, no fertilizer release during plant growth period, strong crop stress resistance (evaluated by superoxide dismutase SOD activity), developed root system, significantly increased total root amount, significantly reduced lodging rate, and somewhat improved corn yield.
Comparative example
This comparative example relates to the effect of organic nitrogen source preparation conditions on self-assembled nitrogen-containing fertilizers.
Comparative example 1
A self-assembly nitrogenous fertilizer, namely a nitrogenous fertilizer-special urea IV, is prepared according to the following method:
in a 2L flask, stirring is started, 500g of water and 500g of catalytic polysuccinimide are added at one time, the polysuccinimide is obtained by an L-aspartic acid phosphoric acid catalytic method, the polymerization degree is 78, and the content of free aspartic acid is<0.1%, phosphoric acid content (in PO) 4 3- 7.62 percent of the total weight of the components, transferring the mixture into a colloid mill by using a pouring method after uniformly stirring, and crushing the mixed material for 90min by using a wet milling method under the condition of 8000-10000 r/min, wherein the material is a non-laminated suspending agent, the particle size of the material is less than or equal to 5 mu m measured by a laser particle sizer, and the solid content of the material is 50 percent.
Uniformly pumping the suspending agent into molten urea (urea is an amide nitrogen source of the synergist and accounts for 40% of the mass of the synergist) according to the condition that the polysuccinimide accounts for 60% of the mass of the synergist, and keeping the material reaction temperature at 100-135 ℃ until no obvious polysuccinimide particles exist in a system to obtain an organic nitrogen source synergist for producing special urea IV; the synergist is added into molten urea slurry for spraying granulation after being evenly stirred according to 20 kg/ton of synergist, 3.0 kg/ton of 3, 4-dimethylpyrazole phosphate (DMPP) and 0.5 kg/ton of allantoin to form the special urea IV. 45.50% of total nitrogen in the special urea IV meets the relevant regulation of the national standard GB/T2440-2017 urea; meanwhile, the composition contains 1.2 percent of protein-bound nitrogen, 0.2 percent of DMPP and 0.05 percent of allantoin.
Performing topdressing field test of summer corn on the special urea IV, the common fertilizer and the special urea I, wherein the special urea IV treatment is a constant fertilization test, the using amount is 15 kg/mu, and the special urea IV treatment is performedCompared with the topdressing amount of 15 kg/mu of common fertilizer and the topdressing amount of 15 kg/mu of special urea I, each treatment is repeated for 3 times, and the area of each cell is 300m 2 Each cell performs a random block. The test conditions and operation, data statistics and analysis methods are the same as those of example 1; the results after combining the data are shown in Table 4 below.
Figure BDA0003724133150000111
The final nitrogen utilization rate of the special urea IV is improved, the plants do not lose fertilizer in the growth period, the stress resistance of the crops is strong (evaluated by the activity of superoxide dismutase SOD), the root system is developed, the total root amount is slightly increased, and the lodging rate is reduced; but the method still has obvious defects compared with the special urea I, and all detection index values are obviously weaker than the special urea I, wherein the most obvious is the difference between the total number of roots and the number of fibrous roots, and the difference is more than 20%; the visual expression is that the growth of the crops in the seedling stage is not obviously increased, and the data display difference exceeds 10%.
Comparative example 2
A self-assembly nitrogenous fertilizer, namely a nitrogenous fertilizer-special urea V, is prepared according to the following method:
stirring is started in a 2L flask, 500g of water and 500g of polysuccinimide are added at one time, the polysuccinimide is obtained by an L-aspartic acid thermal polymerization method (the thermal polymerization temperature is 250 +/-5 ℃, the thermal polymerization time is 6 hours), the polymerization degree is 75, the content of free aspartic acid is less than 0.5 percent, the polysuccinimide is transferred to a colloid mill by a pouring method after being uniform, the mixed material is ground by a wet grinding method under the condition of 8000-10000 r/min, the mixed material is a non-layering suspending agent, the particle size of the material is less than or equal to 5 mu m measured by a laser particle sizer, and the solid content of the material is 50 percent.
Uniformly pumping the suspending agent into molten ammonium carbonate (ammonium carbonate is a nitrogen source of the synergist and is non-amide nitrogen, and the proportion of the ammonium carbonate is 40% of the mass of the synergist) according to the condition that the polysuccinimide accounts for 60% of the mass of the synergist, and keeping the reaction temperature of the materials at 100-135 ℃ until no polysuccinimide particles exist in the system to obtain the organic nitrogen source synergist for producing the special urea V; the synergist is added into molten urine for spraying granulation after being evenly stirred according to 20 kg/ton of synergist, 3.0 kg/ton of 3, 4-dimethylpyrazole phosphate (DMPP) and 0.5 kg/ton of allantoin, thus forming the special urea V. The total nitrogen in the special urea V is 45.50 percent, and meets the relevant regulation of the national standard GB/T2440-2017 urea; meanwhile, the composition contains 1.2 percent of protein-bound nitrogen, 0.3 percent of DMPP and 0.05 percent of allantoin.
Performing topdressing field test of summer corn on the special urea V, the common fertilizer and the special urea I, performing constant fertilization test of the special urea V15 kg/mu, comparing with topdressing amount of the common fertilizer 15 kg/mu and special urea I15 kg/mu, repeating each treatment for 3 times, wherein the area of each cell is 300m 2 Each cell performs a random block. The test conditions and operation, data statistics and analysis methods are the same as those of example 1; the results after combining the data are shown in Table 5 below.
Figure BDA0003724133150000121
The final nitrogen utilization rate of the special urea V is slightly improved, the plants do not lose fertilizer in the growth period, the stress resistance of the crops is strong (evaluated by the activity of superoxide dismutase SOD), the root system is developed, the total root amount is increased to a certain extent, the lodging rate is reduced to a certain extent, and the corn yield is improved to a certain extent; but the indexes are still obviously insufficient compared with the indexes of the special urea I.
Comparative example 3
A self-assembly nitrogenous fertilizer, namely a nitrogenous fertilizer-special urea VI, is prepared according to the following method:
stirring is started in a 2L flask, 500g of water and 500g of polysuccinimide are added at one time, the polysuccinimide is obtained by ammonium (di) maleate thermal polymerization, the polymerization degree is 12, wherein the content of diammonium maleate is 12.76%, after the mixture is uniform, the mixture is transferred into a colloid mill by a pouring method, the mixture is ground for 75min by a wet grinding method under the condition of 8000-10000 r/min, at the moment, the material is a non-stratified suspending agent, the particle size of the material is less than or equal to 5 mu m measured by a laser particle sizer, and the solid content of the material is 50%.
Uniformly pumping the suspending agent into molten urea (urea is an amide nitrogen source of the synergist and accounts for 40% of the mass of the synergist) according to the mass of the polysuccinimide accounting for 60% of the mass of the synergist, and keeping the reaction temperature of the materials at 100-135 ℃ until no polysuccinimide particles exist in the system to obtain the organic nitrogen source synergist for producing the special urea VI; the synergist is added into molten urine for spraying granulation after being evenly stirred according to 20 kg/ton of synergist, 3.0 kg/ton of 3, 4-dimethylpyrazole phosphate (DMPP) and 0.5 kg/ton of allantoin, so as to form the special urea VI. 45.50 percent of total nitrogen in the special urea VI meets the relevant regulation of the national standard GB/T2440-2017 urea; meanwhile, the composition contains 1.2 percent of protein-bound nitrogen, 0.2 percent of DMPP and 0.05 percent of allantoin.
Performing topdressing field test of summer corn on the special urea VI, the common fertilizer and the special urea I, performing constant fertilization test of the special urea VI of 15 kg/mu, comparing with topdressing amount of the common fertilizer of 15 kg/mu and special urea I of 15 kg/mu, repeating each treatment for 3 times, wherein the area of each cell is 300m 2 Each cell performs a random block. The test conditions and operation, data statistics and analysis methods are the same as those of example 1; the results after combining the data are shown in Table 6 below.
Figure BDA0003724133150000131
Figure BDA0003724133150000141
Compared with the common urea, the final nitrogen utilization rate of the special urea VI is almost equal, the stress resistance of crops is slightly enhanced (evaluated by the activity of superoxide dismutase SOD), the development degree of root systems is slightly increased, the total root quantity is increased to a certain extent, the lodging rate is slightly reduced, and the corn yield is slightly improved; but the indexes are still obviously insufficient compared with the indexes of the special urea I.
In conclusion, the self-assembly nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist disclosed by the invention effectively controls and releases nitrogen elements by using the organic nitrogen source, reduces the loss of volatilization, leaching and the like of the conventional nitrogen source, obviously improves the comprehensive utilization rate of the fertilizer in the application process, and promotes the organic implementation of intensive agricultural production.

Claims (10)

1. The nitrogen-fixing fertilizer-maintaining synergist is characterized in that: the synergist is an organic nitrogen source synergist and is mainly formed by reacting polysuccinimide and amide nitrogen, wherein the polymerization degree of the polysuccinimide is 15-80, and the mass of the polysuccinimide accounts for 20-80% of the total mass of the organic nitrogen source synergist.
2. The nitrogen-fixing fertilizer-maintaining synergist of claim 1, characterized in that: the polysuccinimide is obtained by polymerization at a temperature of 180-300 ℃ by a thermal aspartic acid polymerization method, a thermal maleic acid ammonium salt polymerization method or a thermal fumaric acid ammonium salt polymerization method.
3. The nitrogen-fixing fertilizer-maintaining synergist of claim 1, characterized in that: the amide nitrogen is at least one of urea, urea formaldehyde, butylene diurea and amide.
4. The nitrogen-fixing fertilizer-maintaining synergist of claim 1, characterized in that: the organic nitrogen source synergist is mainly prepared by adding fluid polysuccinimide into molten amide nitrogen for reaction.
5. A method for preparing the nitrogen-fixing fertilizer-maintaining synergist as claimed in any one of claims 1-4, characterized in that: the method comprises the steps of preparing the raw material polysuccinimide into a non-layered fluid material, uniformly adding the non-layered fluid material into molten amide nitrogen, keeping the material completely reacted without obvious polysuccinimide, and forming to obtain the synergist.
6. The preparation method of the nitrogen-fixing fertilizer-preserving synergist according to claim 5, characterized in that: processing the mixture by using water as a suspension medium by using a colloid mill or a homogenizer to obtain fluid polysuccinimide; the mass ratio of the polysuccinimide to the water in the process of preparing the fluid polysuccinimide is 1 (0.25-2.50).
7. A self-assembled nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist of any one of claims 1 to 4, which is characterized in that: the nitrogen-containing fertilizer comprises 1-70 parts of nitrogen-fixing and fertilizer-maintaining synergist per hundred parts.
8. The self-assembled nitrogen-containing fertilizer containing nitrogen-fixing and fertilizer-maintaining synergist of claim 7, wherein: the nitrogenous fertilizer also comprises auxiliary materials, and the auxiliary materials comprise at least one of nitrification inhibitor, urease inhibitor and synergistic accelerator.
9. The self-assembled nitrogen-containing fertilizer containing nitrogen-fixing and fertilizer-maintaining synergist of claim 8, wherein: the nitrification inhibitor is at least one of 2-chloro-6- (trichloromethyl) pyridine and 3, 4-dimethylpyrazole phosphate, and each hundred parts of nitrogen-containing fertilizer comprises 0.1-5.0 parts of nitrification inhibitor;
the urease inhibitor is a phosphorus amine urease inhibitor, and each hundred parts of nitrogen-containing fertilizer comprises 0.5-5.0 parts of urease inhibitor;
the synergistic accelerator is at least one of allantoin, polyamine substances, oligosaccharins and jasmonic acid substances, and each hundred parts of nitrogen-containing fertilizer comprises 0.05-1.0 part of synergistic accelerator.
10. A method for preparing the self-assembled nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist as defined in claim 8 or 9, which is characterized in that: uniformly stirring the nitrogen-fixing and fertilizer-maintaining synergist and the auxiliary materials, and adding the mixture into the production process of the common nitrogen-containing fertilizer according to a proportion to obtain the self-assembly nitrogen-containing fertilizer containing the nitrogen-fixing and fertilizer-maintaining synergist.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105482117A (en) * 2016-01-19 2016-04-13 北京理工大学 Polyaspartic acid/urea graft copolymer as well as preparation method and application thereof
CN110357709A (en) * 2019-07-09 2019-10-22 中国农业科学院作物科学研究所 A kind of corn resistance physiology slow release fertilizer synergist and the preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105482117A (en) * 2016-01-19 2016-04-13 北京理工大学 Polyaspartic acid/urea graft copolymer as well as preparation method and application thereof
CN110357709A (en) * 2019-07-09 2019-10-22 中国农业科学院作物科学研究所 A kind of corn resistance physiology slow release fertilizer synergist and the preparation method and application thereof

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